data_5s_mcm20b-p-1 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C24 H46 Cl2 P2 Pt' _chemical_formula_sum 'C24 H46 Cl2 P2 Pt' _chemical_formula_weight 662.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7585(16) _cell_length_b 7.8401(16) _cell_length_c 11.023(2) _cell_angle_alpha 96.88(3) _cell_angle_beta 102.46(3) _cell_angle_gamma 97.12(3) _cell_volume 642.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7666 _cell_measurement_theta_min 2.6485 _cell_measurement_theta_max 27.4815 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.302 _exptl_crystal_size_mid 0.288 _exptl_crystal_size_min 0.243 _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method none _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 5.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.240 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick, 2003)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'glass fibre' _diffrn_radiation_collimation monocap _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size ? _diffrn_source_target Mo _diffrn_source_type ? _diffrn_source_voltage 50 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8243 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2941 _reflns_number_gt 2941 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction ; SAINT v7.06A (Bruker-AXS, 1997-2003) & SHELXTL v6.14 (Bruker-AXS, 2003) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Following initial refinement an isolated electron density peak was found in the difference map 2.3 Angstroms from the chlorine ligand and 0.55 Angstroms from a special position. Several possible scenarios that might explain this feature were investigated. One possiblility is that this peak is due to water molecule. However, the water would be too close to the chlorine to make a sensible hydrogen bond. Refinement using this model was attempted with an occupancy of 0.5 but anisotropic refinement of the thermal parameters of the oxygen atom proved difficult and subsequent refinement of occupancy caused the thermal parameters to produce a non-positive definate. A second possibility is that the crystal contains a slight degree of whole-molecule disorder. Assigning the peak as a second Pt atom and contraining the sum of occupancies of the Pt atoms of the two complexes to gave a satisfactory refinement, the results of which are presented here. The near identical lengths of the a and b axes may indicate the possibility of twinning with the components related by 2-fold rotation about a vector that bisects these axes. Unfortunately, by the time this was recognised, the image data were no longer available to fully investigate this possibility. Using a twin matrix that gives a 2-fold rotation about the bisector of the h and k axes gave a refinement that converged but had no significant effect on the residuals. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2941 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0148 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0367 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.0000 0.0000 0.00923(4) Uani 0.9711(8) 2 d SP . 1 P1 P 0.36154(7) 0.19686(6) 0.10317(5) 0.01277(11) Uani 1 1 d . A 1 Cl1 Cl 0.27674(7) -0.22277(6) 0.00111(5) 0.01732(11) Uani 1 1 d . B 1 C1 C 0.2037(3) 0.2906(3) -0.00971(19) 0.0172(4) Uani 1 1 d . A 1 H1A H 0.0828 0.2645 0.0057 0.021 Uiso 1 1 calc R A 1 H1B H 0.2381 0.4186 0.0049 0.021 Uiso 1 1 calc R A 1 C2 C 0.1969(3) 0.2219(3) -0.14726(18) 0.0171(4) Uani 1 1 d . A 1 H2A H 0.3177 0.2478 -0.1628 0.021 Uiso 1 1 calc R A 1 H2B H 0.1620 0.0940 -0.1621 0.021 Uiso 1 1 calc R A 1 C3 C 0.0653(3) 0.3015(3) -0.24013(19) 0.0192(4) Uani 1 1 d . A 1 H3A H 0.0997 0.4295 -0.2255 0.023 Uiso 1 1 calc R A 1 H3B H -0.0559 0.2748 -0.2254 0.023 Uiso 1 1 calc R A 1 C4 C 0.0621(4) 0.2312(3) -0.3768(2) 0.0271(5) Uani 1 1 d . A 1 H4A H 0.1819 0.2576 -0.3917 0.041 Uiso 1 1 calc R A 1 H4B H -0.0219 0.2861 -0.4337 0.041 Uiso 1 1 calc R A 1 H4C H 0.0241 0.1050 -0.3924 0.041 Uiso 1 1 calc R A 1 C5 C 0.5111(3) 0.3751(3) 0.21569(19) 0.0165(4) Uani 1 1 d . A 1 H5 H 0.5841 0.4426 0.1679 0.020 Uiso 1 1 calc R A 1 C6 C 0.4047(3) 0.5007(3) 0.2759(2) 0.0204(4) Uani 1 1 d . A 1 H6A H 0.4907 0.5955 0.3334 0.024 Uiso 1 1 calc R A 1 H6B H 0.3342 0.5540 0.2086 0.024 Uiso 1 1 calc R A 1 C7 C 0.2780(3) 0.4206(3) 0.3492(2) 0.0218(4) Uani 1 1 d . A 1 H7A H 0.2026 0.5071 0.3710 0.026 Uiso 1 1 calc R A 1 H7B H 0.3495 0.3946 0.4288 0.026 Uiso 1 1 calc R A 1 C8 C 0.1552(3) 0.2521(3) 0.2775(2) 0.0212(4) Uani 1 1 d . A 1 H8A H 0.0929 0.1995 0.3366 0.025 Uiso 1 1 calc R A 1 H8B H 0.0630 0.2842 0.2106 0.025 Uiso 1 1 calc R A 1 C9 C 0.2473(3) 0.1126(3) 0.21666(19) 0.0177(4) Uani 1 1 d . A 1 H9 H 0.1524 0.0141 0.1705 0.021 Uiso 1 1 calc R A 1 C10 C 0.3868(3) 0.0377(3) 0.3098(2) 0.0228(5) Uani 1 1 d . A 1 H10A H 0.4274 -0.0585 0.2620 0.027 Uiso 1 1 calc R A 1 H10B H 0.3263 -0.0132 0.3705 0.027 Uiso 1 1 calc R A 1 C11 C 0.5541(3) 0.1663(3) 0.3852(2) 0.0233(5) Uani 1 1 d . A 1 H11A H 0.5205 0.2370 0.4545 0.028 Uiso 1 1 calc R A 1 H11B H 0.6451 0.0982 0.4236 0.028 Uiso 1 1 calc R A 1 C12 C 0.6398(3) 0.2901(3) 0.3091(2) 0.0209(4) Uani 1 1 d . A 1 H12A H 0.7114 0.2246 0.2614 0.025 Uiso 1 1 calc R A 1 H12B H 0.7236 0.3840 0.3690 0.025 Uiso 1 1 calc R A 1 PtX Pt 0.0507(7) -0.4436(7) -0.0014(5) 0.0136(17) Uani 0.0145(4) 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01022(6) 0.00824(6) 0.00929(6) 0.00167(4) 0.00205(4) 0.00171(4) P1 0.0144(2) 0.0125(2) 0.0115(2) 0.00205(18) 0.00278(19) 0.00299(19) Cl1 0.0173(2) 0.0135(2) 0.0212(2) 0.00111(18) 0.00753(19) -0.00145(18) C1 0.0186(10) 0.0195(10) 0.0140(9) 0.0028(7) 0.0021(8) 0.0072(8) C2 0.0193(10) 0.0183(10) 0.0132(9) 0.0025(7) 0.0010(8) 0.0057(8) C3 0.0200(11) 0.0201(10) 0.0174(10) 0.0046(8) 0.0013(8) 0.0058(8) C4 0.0313(13) 0.0334(13) 0.0167(10) 0.0044(9) 0.0020(9) 0.0107(10) C5 0.0183(10) 0.0154(9) 0.0148(9) 0.0009(7) 0.0028(8) 0.0024(8) C6 0.0257(12) 0.0169(10) 0.0170(10) -0.0014(8) 0.0027(8) 0.0055(9) C7 0.0267(12) 0.0243(11) 0.0164(10) 0.0010(8) 0.0066(9) 0.0107(9) C8 0.0228(11) 0.0258(11) 0.0176(10) 0.0039(8) 0.0082(8) 0.0075(9) C9 0.0196(11) 0.0182(10) 0.0165(10) 0.0034(8) 0.0068(8) 0.0019(8) C10 0.0313(13) 0.0224(11) 0.0175(10) 0.0079(8) 0.0072(9) 0.0071(9) C11 0.0277(12) 0.0275(12) 0.0155(10) 0.0048(8) 0.0019(9) 0.0108(9) C12 0.0187(11) 0.0239(11) 0.0175(10) -0.0006(8) -0.0004(8) 0.0045(9) PtX 0.006(3) 0.017(3) 0.018(3) 0.0052(19) 0.0040(18) -0.0011(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.3054(9) 2_655 ? Pt1 Cl1 2.3054(9) . ? Pt1 P1 2.3124(8) . ? Pt1 P1 2.3124(8) 2_655 ? P1 C9 1.822(2) . ? P1 C1 1.837(2) . ? P1 C5 1.843(2) . ? C1 C2 1.534(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.529(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.535(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.541(3) . ? C5 C12 1.545(3) . ? C5 H5 1.0000 . ? C6 C7 1.525(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.546(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.543(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.547(3) . ? C9 H9 1.0000 . ? C10 C11 1.550(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.537(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? PtX PtX 1.116(11) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pt1 Cl1 180.00(3) 2_655 . ? Cl1 Pt1 P1 89.37(3) 2_655 . ? Cl1 Pt1 P1 90.63(3) . . ? Cl1 Pt1 P1 90.63(3) 2_655 2_655 ? Cl1 Pt1 P1 89.37(3) . 2_655 ? P1 Pt1 P1 180.00(3) . 2_655 ? C9 P1 C1 109.05(10) . . ? C9 P1 C5 95.79(10) . . ? C1 P1 C5 108.81(10) . . ? C9 P1 Pt1 115.35(7) . . ? C1 P1 Pt1 110.82(7) . . ? C5 P1 Pt1 115.99(7) . . ? C2 C1 P1 113.35(14) . . ? C2 C1 H1A 108.9 . . ? P1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C1 112.75(17) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2 C3 C4 111.61(18) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C6 C5 C12 115.26(17) . . ? C6 C5 P1 111.50(15) . . ? C12 C5 P1 106.91(14) . . ? C6 C5 H5 107.6 . . ? C12 C5 H5 107.6 . . ? P1 C5 H5 107.6 . . ? C7 C6 C5 115.85(18) . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C5 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 114.01(18) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 116.28(19) . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C7 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C8 C9 C10 115.10(18) . . ? C8 C9 P1 111.31(15) . . ? C10 C9 P1 106.70(15) . . ? C8 C9 H9 107.8 . . ? C10 C9 H9 107.8 . . ? P1 C9 H9 107.8 . . ? C9 C10 C11 116.72(18) . . ? C9 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C9 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C12 C11 C10 115.50(18) . . ? C12 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? C11 C12 C5 116.64(19) . . ? C11 C12 H12A 108.1 . . ? C5 C12 H12A 108.1 . . ? C11 C12 H12B 108.1 . . ? C5 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pt1 P1 C9 -145.38(8) 2_655 . . . ? Cl1 Pt1 P1 C9 34.62(8) . . . . ? Cl1 Pt1 P1 C1 90.11(9) 2_655 . . . ? Cl1 Pt1 P1 C1 -89.89(9) . . . . ? Cl1 Pt1 P1 C5 -34.58(8) 2_655 . . . ? Cl1 Pt1 P1 C5 145.42(8) . . . . ? C9 P1 C1 C2 -128.52(16) . . . . ? C5 P1 C1 C2 128.17(16) . . . . ? Pt1 P1 C1 C2 -0.50(18) . . . . ? P1 C1 C2 C3 -179.85(15) . . . . ? C1 C2 C3 C4 179.68(19) . . . . ? C9 P1 C5 C6 -59.69(16) . . . . ? C1 P1 C5 C6 52.71(17) . . . . ? Pt1 P1 C5 C6 178.43(12) . . . . ? C9 P1 C5 C12 67.11(16) . . . . ? C1 P1 C5 C12 179.52(14) . . . . ? Pt1 P1 C5 C12 -54.77(15) . . . . ? C12 C5 C6 C7 -62.4(3) . . . . ? P1 C5 C6 C7 59.7(2) . . . . ? C5 C6 C7 C8 -48.9(3) . . . . ? C6 C7 C8 C9 48.8(3) . . . . ? C7 C8 C9 C10 62.2(3) . . . . ? C7 C8 C9 P1 -59.4(2) . . . . ? C1 P1 C9 C8 -53.01(18) . . . . ? C5 P1 C9 C8 59.20(17) . . . . ? Pt1 P1 C9 C8 -178.43(12) . . . . ? C1 P1 C9 C10 -179.34(14) . . . . ? C5 P1 C9 C10 -67.13(16) . . . . ? Pt1 P1 C9 C10 55.24(16) . . . . ? C8 C9 C10 C11 -63.9(3) . . . . ? P1 C9 C10 C11 60.2(2) . . . . ? C9 C10 C11 C12 -43.8(3) . . . . ? C10 C11 C12 C5 43.6(3) . . . . ? C6 C5 C12 C11 65.0(3) . . . . ? P1 C5 C12 C11 -59.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.079 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.098